Category: 460-37-7

Synthetic Route of 460-37-7, Catalysts allow a reaction to proceed via a pathway that has a lower activation energy than the uncatalyzed reaction. 460-37-7, Name is 1,1,1-Trifluoro-3-iodopropane, SMILES is ICCC(F)(F)F, belongs to iodides-buliding-blocks compound. In a article, author is Chambers, RD, introduce new discover of the category.

New fluorocarbon iodides

A general, efficient approach for the synthesis of fluorocarbon iodides and di-iodides bearing hydrocarbon groups is described and the synthetic utility of these new systems is demonstrated in reactions with thiols.

Synthetic Route of 460-37-7, The reactant in an enzyme-catalyzed reaction is called a substrate. Enzyme inhibitors cause a decrease in the reaction rate of an enzyme-catalyzed reaction.I hope my blog about 460-37-7 is helpful to your research.

Chemistry is the experimental and theoretical study of materials on their properties at both the macroscopic and microscopic levels. 460-37-7, Name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I. In an article, author is Kirihara, Masayuki,once mentioned of 460-37-7, Category: iodides-buliding-blocks.

Deprotection of dithioacetals with 30% hydrogen peroxide catalyzed by tantalum(V) chloride-sodium iodide or niobium(V) chloride-sodium iodide

The reaction of dithioacetals with 30% hydrogen peroxide in the presence of catalytic amounts of tantalum(V) and iodide ion effectively produced carbonyl compounds in high yields. Dithioacetals also can be deprotected using the niobium(V) catalyzed oxidation of iodide ion by hydrogen peroxide under mild conditions. (C) 2011 Elsevier Ltd. All rights reserved.

If you¡¯re interested in learning more about 460-37-7. The above is the message from the blog manager. Category: iodides-buliding-blocks.

Adding a certain compound to certain chemical reactions, such as: 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 460-37-7, Safety of 1,1,1-Trifluoro-3-iodopropane

A THF (75 mL) suspension of Zn (from Aldrich, dust, 325 mesh, 30.0 g, 461 mmol) was stirred under N2 at ambient temperature for 10 min. Afterward, 1,2-dibromoethane (from Aldrich, 4.75 g, 25.3 mmol) was added. The resulting mixture was brought to reflux times with a heat gun under N2, and then cooled to ambient temperature in a water bath. These reflux and cooling steps were repeated two more times. The mixture was then cooled to 0C in an ice bath. Chlorotrimethylsilane (from Aldrich, 3.42 mL, 26.9 mmol) was slowly added to the cooled mixture over a period of a few minutes. The resulting mixture was stirred at 0C for 5 min, and then allowed to warm to ambient temperature over 15 min while continuing to be stirred. Afterward, the mixture was cooled to 0C, and then slowly treated with 1, 1, L-TRIFLUORO-3-IODOPROPANE causing an exothermic reaction. The mixture was warmed to ambient temperature and stirred for 1 hr. The mixture was then diluted with N, N-dimethylacetamide (10 mL) to afford an organozinc reagent. Separately, an N, N-dimethylacetamide (40 mL) solution of the product from Part E (2.0 g, 3.3 mmol) was treated with bis (benzonitrile) dichloropalladium (II) (from Aldrich, 0.08 g, 0.208 mmol) and 2- (DICYCLOHEXYLPHOSPHINO)-2′-METHYLBIPHENYL (0.127 g, 0.349 mmol) under N2. The organozinc reagent (2.2 mL of stock solution, 9.78 mmol) was then added to the mixture. The resulting mixture was stirred at 55C for 4 hr, and then allowed to cool to ambient temperature overnight. Subsequently, the reaction was quenched with saturated aqueous NAHC03 (20 mL). The mixture was then partitioned further with ethyl acetate (100 mL) and de-ionized water (50 mL). The resulting biphasic mixture was filtered through Celite (pre-washed with ethyl acetate). The filter cake, in turn, was washed with ethyl acetate. The organic layer was separated, and the aqueous layer was extracted with ethyl acetate (50 mL). The combined organic layers were washed with saturated aqueous NAHCO3 (2×25 mL), washed with 1: 1 brine/de-ionized water (2×25 mL), washed with brine (2×25 mL), dried over NA2S04, filtered, and concentrated in vacuo. The resulting solid was diluted in diethyl ether, and then concentrated in VACUO, FORMING a glassy solid. This solid was triturated with 1: 1 diethyl ETHER/HEXANES. The solids were then filtered, washed with hexanes, and dried in a vacuum oven to afford the desired ester as a brown solid (1.25 g, 76% yield). The presence of the desired ester was confirmed BY 1HU R AND L9F-NMR. LC/MS m/z = 500 [M+H], 522 [M+NA].

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1,1,1-Trifluoro-3-iodopropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; PHARMACIA CORPORATION; WO2004/48368; (2004); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 460-37-7,Some common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To stirred a solution of methyl-(2S)-2-(te/Y-butoxycarbonyl)-amino-2-[8-aza-bicyclo [3.2.1]-oct-3-yl]-exo-acetate (step 5 of intermediate 2, 1.0 g, 3.36 mmol) in acetonitrile (20 ml) at room temperature was added anhydrous K2CO3 (1.39g, 10.07 mmol) stirred for 10 minutes. To this reaction mixture was then added 3,3,3-trifluoropropyl iodide (0.827g, 0.43 ml, 3.69 mmol) and heated at 5O0C for 6 hours under stirring. The solvent was removed under reduced pressure and added ethyl acetate (50 ml). The organic layer was washed with water (2×20 ml), bromine (10 ml) and dried over anhydrous Na2SO4. The solvent was evaporated to yield the crude product, which was purified by column chromatography over silica gel (100-200 mesh) using 1.3% methanol in dichloromethane as an eluent to yield the title compound (0.775g, 58%). MS: m/z 395(M+1) 1HNMR (CDCI3, 200 MHz): delta 1.17-1.60 (m, 15H), 1.82-2.40 (m, 5H), 2.5 -2.63 (m, 2H), 3.14- 3.28 (m, 2H) 3.73 (s, 3H) 4.10-4.30 (m, 1 H), 4.97-5.10 (m, 1 H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,1,1-Trifluoro-3-iodopropane, its application will become more common.

Reference:
Patent; LUPIN LIMITED; WO2009/37719; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 460-37-7, These common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Example 1 2-Bromo-4-methyl-5-[(2,3,6-trifluorophenyl)[(3,3,3-trifluoropropyl)thio]methyl]pyridine Sodium hydride (60 mg, 1.38 mmol) and 1,1,1-trifluoro-3-iodopropane (165 mul, 1.38 mmol) were added to a N,N-dimethylformamide (5 ml) solution of (6-bromo-4-methylpyridin-3-yl)(2,3,6-trifluorophenyl)methanethiol (400 mg, 1.15 mmol) at 0 C., and the solution was stirred at room temperature for 2 hours. Water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was washed sequentially with water and saturated saline. The resulting organic layer was dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The resulting residue was subjected to flash silica gel column chromatography (hexane/ethyl acetate) to give the title compound (390 mg, 0.878 mmol, 76%) as a yellow oil. 1H-NMR (400 MHz, CDCl3) delta: 2.23 (3H, s), 2.29-2.46 (2H, m), 2.65-2.77 (2H, m), 5.48 (1H, s), 6.84-6.90 (1H, m), 7.08-7.16 (1H, m), 7.28 (1H, s), 8.79 (1H, s). MS (m/z): 444 (M++H).

Statistics shows that 1,1,1-Trifluoro-3-iodopropane is playing an increasingly important role. we look forward to future research findings about 460-37-7.

Reference:
Patent; DAIICHI SANKYO COMPANY, LIMITED; US2010/168136; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, A new synthetic method of this compound is introduced below., Computed Properties of C3H4F3I

General procedure: 2-Thioadenosine (300 mg, 1 mmol) was dissolved with stirring in 7.5 ml DMF. Sodium dithionite (750 mg) was added and the mixture was stirred for 30 min under Ar. The reaction mixture was cooled in ice, aqueous sodium hydroxide (50% (w/w) solution (240 mg, 3 mmol) was added, and after 10 min stirring the alkyl iodide (1.1 mmol) was added dropwise over 10 min. The cooling was removed, and after 1 h stirring at rt the reaction mixture was analyzed by LCMS. If unreacted starting material was present an additional amount of alkyl iodide (0.134 mmol, 0.2 eqv.) was added with ice cooling, and after 1 h stirring at room temperature the analysis was repeated. When no starting material was present the reaction mixture was diluted with 75 ml of water and after ca. 2 h stirring the crude product was collected by filtration and washed with water. This material was purifiedby column chromatography on silica gel using chloroform/methanol as eluent.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Article; Yanachkov, Ivan B.; Chang, Hung; Yanachkova, Milka I.; Dix, Edward J.; Berny-Lang, Michelle A.; Gremmel, Thomas; Michelson, Alan D.; Wright, George E.; Frelinger, Andrew L.; European Journal of Medicinal Chemistry; vol. 107; (2016); p. 204 – 218;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Product Details of 460-37-7

1,2-Dibromoethane (0.04 ml, 0.51 mmol) was added to a stirred suspension of zinc (0.45 g, 6.82 mmol) in DMF (3.5 ml). The mixture was stirred at 90 C for 30 min. under nitrogen and then chlorotrimethylsilane (0.013 ml, 0.102 mmol) was added. The mixture was stirred at RT for a further 30 min. and then a solution of 3-iodo-l,l,l- trifluoropropane in DMF (2 ml) was added dropwise . The mixture was stirred at 45 C for 2.5 h. and the resulting solution was transferred via syringe to a second flask charged with intermediate 34 (0.144 g, 0.34 mmol) andbis(triphenylphosphine)palladium (II) dichloride (0.024 g, 0.034 mmol) under nitrogen. The mixture was stirred at 40 C for 1 h. and then allowed to cool down to RT. A saturated solution of ammonium chloride was added and the mixture was extracted with EtOAc. The organic layer was separated, washed with a saturated solution of ammonium chloride and brine, dried (Na2S04), filtered and the solvents evaporated in vacuo. The crude product was purified by flash column chromatography (silica; EtOAc in heptane 0/100 to 100/0). The desired fractions were collected and evaporated in vacuo to yield intermediate 38 (0.07 g, 52%) as a pale brown solid.

The synthetic route of 460-37-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; BARTOLOME-NEBREDA, Jose, Manuel; CONDE-CEIDE, Susana; MACDONALD, Gregor, James; PASTOR-FERNANDEZ, Joaquin; VAN GOOL, Michiel, Luc, Maria; MARTIN-MARTIN, Maria, Luz; VANHOOF, Greta, Constantia, Peter; WO2011/110545; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: 1,1,1-Trifluoro-3-iodopropane

Example 296A 3-(2-Methoxyethyl)-5-methyl-2,4-dioxo-1-(3,3,3-trifluoropropyl)-1,2,3,4-tetrahydrothieno[2,3-d]pyrimidine-6-carbaldehyde 341 mg (2.47 mmol) of potassium carbonate were added to a solution of 285 mg (0.98 mmol) of the compound from Ex. 53A in 9 ml of DMF, and the mixture was stirred at RT for 15 min. Then 664 mg (2.96 mmol) of 1,1,1-trifluoro-3-iodopropane were added, and the mixture was stirred at 50 C. for 19 h. The DMF was then very substantially distilled off and the remaining residue was partitioned between semisaturated sodium chloride solution (200 ml) and ethyl acetate (100 ml). The aqueous phase was extracted with ethyl acetate. The combined organic phases were dried over sodium sulphate, filtered and concentrated. The residue obtained was chromatographed using a silica gel cartridge (Biotage, 50 g of silica gel, eluent: hexane/ethyl acetate). 254 mg (69% of theory) of the title compound were obtained. 1H-NMR (400 MHz, DMSO-d6, delta/ppm): 10.11 (s, 1H), 4.18 (t, 2H), 4.06 (t, 2H), 3.53-3.48 (m, 2H), 3.24 (s, 3H), 2.84-2.75 (m, 5H). LC/MS (Method 3, ESIpos): Rt=1.10 min, m/z=365 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 460-37-7, its application will become more common.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HAeRTER, Michael; KOSEMUND, Dirk; DELBECK, Martina; KALTHOF, Bernd; WASNAIRE, Pierre; SUessMEIER, Frank; LUSTIG, Klemens; (369 pag.)US2018/65981; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 460-37-7,Some common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Methyl 1H-1,2,4-triazole-3-carboxylate (8.11 g, 63.8 mmol) was dissolved in N,Ndimethylformamide (41 ml) and cooled to 0C. Sodium hydride (3.32 g, 60% purity, 82.9 mmol) was added and the reaction mixture was stirred for 30 mm at 0C. After i,i,i-trifluoro-3- iodopropane (15.0 g, 67.0 mmol) was added and the resulting mixture was stirred for 16 h at room temperarture. Saturated ammonium chloride solution and ethyl acetate were added. Layers were separated and aqueous layer was extracted with ethyl acetate. Combined organic extracts werewashed with brine, dried over sodium sulfate and solvents were removed in vacuo. The crude product was purified by preparative HPLC (Method 5). Lyophilisation of the product containing fractions afforded 2.56 g (18% of th.) of the title compound1H-NMR (400 MHz, DMSO-d6) [ppm]: 2.904 (0.96), 2.921 (2.07), 2.932 (2.97), 2.938 (1.52),2.948 (5.97), 2.959 (3.22), 2.966 (3.45), 2.976 (5.83), 2.987 (1.41), 2.993 (3.06), 3.004 (1.93),3.021 (0.94), 3.331 (1.18), 4.556 (8.10), 4.573 (16.00), 4.590 (7.72), 8.776 (11.85).

The synthetic route of 460-37-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; COLLIN-KROePELIN, Marie-Pierre; KOLKHOF, Peter; NEUBAUER, Thomas; FUeRSTNER, Chantal; POOK, Elisabeth; TINEL, Hanna; SCHMECK, Carsten; WASNAIRE, Pierre; SCHIRMER, Heiko; LUSTIG, Klemens; (205 pag.)WO2019/81299; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 460-37-7,Some common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Example 168A Ethyl 3-ethyl-2,4-dioxo-5-(trifluoromethyl)-1-(3,3,3-trifluoro9propyl)-1,2,3,4-tetrahydrothieno[2,3-d]pyrimidine-6-carboxylate 1.39 g (13.1 mmol) of caesium carbonate were added to a solution of 2.0 g (5.95 mmol) of the compound from Ex. 165A in 40 ml of DMF, and the mixture was stirred at RT for 15 min. Then 2.66 g (11.9 mmol) of 3,3,3-trifluoro-1-iodopropane were added, and the mixture was heated at 60 C. After 1 h, a further 2.66 g (11.9 mmol) of 3,3,3-trifluoro-1-iodopropane were added. Stirring at 60 C. was continued for 16 h. After cooling to RT, about 160 ml of water were added and the mixture was extracted three times with about 80 ml of diethyl ether each time. The combined organic extracts were washed with saturated sodium chloride solution. After drying over anhydrous magnesium sulphate, the mixture was filtered and the filtrate was evaporated. The crude product was purified by MPLC on a Puriflash cartridge (100 g of silica gel, cyclohexane/ethyl acetate 7:1?1:1). The product fractions were combined and concentrated, and the residue was dried under high vacuum. 1.86 g (72% of theory) of the title compound were obtained. 1H-NMR (400 MHz, CDCl3, delta/ppm): 4.41 (q, 2H), 4.20 (t, 2H), 4.08 (q, 2H), 2.73-2.61 (m, 2H), 1.40 (t, 3H), 1.26 (t, 3H). LC/MS (Method 1, ESIpos): Rt=1.15 min, m/z=433 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,1,1-Trifluoro-3-iodopropane, its application will become more common.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HAeRTER, Michael; KOSEMUND, Dirk; DELBECK, Martina; KALTHOF, Bernd; WASNAIRE, Pierre; SUessMEIER, Frank; LUSTIG, Klemens; (369 pag.)US2018/65981; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com